Selda Mercan

Quantitative lead determination in coating paint on children׳s outwear by LA-ICP-MS: A practical calibration strategy for solid samples

Lead is a hazardous compound that affects the central nervous system in people, particularly children, and may cause some reversible and irreversible diseases. Legal regulations try to prevent the exposure from products especially produced for children such as coating paints, jewelry, toys, bed linen, textile, etc. The aim of this study was to determine the lead levels of coating paints on children׳s outwear selling in district bazaar by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and to specify the percent of non-complying samples. Here we described the solid matrix calibration method and confirmed the results with the microwave-assisted acid digestion method. Both comparative methods were validated by analysis of the certified reference materials (NIST SRM-612 glass matrix, NIST SRM-2582 powdered paint and ERM-EC681k) and bias% for accuracy and RSD% for precision were calculated lower than 6.8% and 7.3%, respectively. The recovery ranges of laser ablation and microwave-assisted acid digestion method for Pb were found to be between 88.2-98.1% and 95.3-101.3%, respectively. The limits of detection values were determined as 0.162 mg kg(-1) for direct sampling in the ablation chamber and 0.002 ng mL(-1) for aqueous solutions. Correlation result of 16 samples (r=0.99) examined in both methods was satisfactory. In coating paint samples, 14.65% of 198 (n=29) did not comply with the 90 mg kg(-1) lead limit according to regulation. Validated quantitative laser ablation method may be preferred to quickly and reliably determine the Pb levels in other solid samples as well as coating paints.

Elemental composition of green coffee and its contribution to dietary intake

The concentration of twenty-seven elements (Li, Be, B, Mg, Al, P, K, Ca, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Cd, Sn, Sb, Ba, Hg, Pb, Bi, Th, and U) in green coffee samples and their infusions were determined by using inductively coupled plasma-mass spectrometry (ICP-MS). Prior to analysis, green coffee samples were prepared by microwave digestion, while infusions were analyzed without any pre-treatment. The accuracy and precision of the proposed methods were verified by recovery experiments. Considering samples; K, Cu, and Al had the highest mean concentrations with 6714.5μgg(-1), 12.1μgg(-1), and 25.9μgg(-1) among major, trace and toxic elements, respectively. The impact of brewing type on leachability of elements was also studied and the results outlined that mean leachability of elements to Turkish coffee were greater than to mud coffee. Furthermore, dietary element intakes through green coffee consumption were also estimated. This is the first study presenting wide range of elements in green coffee brews and calculating dietary intakes.

Titanium Element Level in Peri-Implant Mucosa

ABSTRACT Although titanium is a highly inert material, it may corrode when in contact with the oral cavity. This study aimed to examine the titanium presence and levels in gingiva samples that had been in contact with a dental implant cover screw for 3 months. Twenty two-staged dental implants were included in the study as a test group. Gingiva samples were taken over the implant sites. Ten control samples were obtained from oral mucosa during gingivoplasty. All samples were analyzed by Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry. The results showed that the average semi-quantitative titanium levels were higher in the test group (50.4 μg/g ± 23.5 μg/g) than in the control group (37.1 μg/g ± 1.0 μg/g). This difference was found to be statistically insignificant (p = 0.075). The presented study showed that titanium may corrode in a relatively short time. Long-term studies are needed with a higher number of patients and varying conditions to evaluate the titanium levels in the soft tissues around implants.

Determination of α-cypermethrin from soil by using HPTLC

α-Cypermethrin is a synthetic pyrethroid insecticide used to control insects. In soil, α-cypermethrin biodegrades relatively slowly under both aerobic and anaerobic conditions. A high-performance thinlayer chromatography (HPTLC) method was developed for the determination of α-cypermethrin from soil by microwave-assisted extraction (MAE). The linearity range was between 12.5 and 1000 ng/spot, the limit of detection was 2.1 ng/spot, the limit of quantification was 6.4 ng/spot, and the recovery was 91%. The reported method was found to be sensitive, rapid, and suitable for the analysis of α-cypermethrin in soil and it was successfully applied to the soil samples collected from a treated agricultural field. α-Cypermethrin was detected in all soil samples at concentrations ranging from 78.9 to 708.7 ng g−1.

An HPTLC Method for the Determination of Oleandrin in Nerium Plant Extracts and Its Application to Forensic Toxicology

The study reported in this paper was aimed to develop an accurate, specific, and precise high-performance thin-layer chromatography (HPTLC) method for the determination of oleandrin in Nerium oleander (Linn.) extracts as well as biological samples of an intoxication case for the first time. Also, extraction, isolation, and purification methods of oleandrin from the sticky juice of Nerium plant leaves were presented. The retention factor (RF value) of oleandrin was found to be 0.24 ± 0.01. The linearity range was between 2 and 75 ng spot−1 (r = 0.9993), the limit of detection was 2.2 ng spot−1, the limit of quantification was 6.7 ng spot−1, and the recovery in urine and serum was found 89% and 83%, respectively. Isolated compounds from both plant material and biological samples were also applied to mass spectrometry (MS). The reported HPTLC method was sensitive, rapid, and suitable for the analysis of oleandrin and was applied to a non-fatal case of oleander poisoning. Oleandrin was detected in urine and serum samples of the intoxicated patient at concentrations of 3.2 and 8.4 ng mL−1, respectively. Peak purity of the isolated compound was checked by electrospray ionization-mass spectrometry (EI-MS) and introduced to HPTLC compound library. To the best of our knowledge, this study is the first published HPTLC method and also presents the evaluation of both clinical and toxicological aspect of an oleander posioning case. It can be successfully applied for the determination of oleandrin in clinical and forensic researches as well as in phytochemical investigations.

Development and validation of a densitometric-high-performance thin-layer chromatographic method for quantitative analysis of amitriptyline in gastric lavage

Drug overdose is the most common method in suicide attempts. Amitriptyline (AMT), a tricyclic antidepressant agent, known for potentially lethal cardiovascular and neurological effects, is used especially by intoxicated patients. The aim of this study was to validate a method for the determination of AMT in gastric lavage samples by high-performance thin-layer chromatography (HPTLC). Artificial gastric lavage was used to obtain a better extraction procedure for AMT. The method was also applied to patients who attempted suicide with AMT. A validated, accurate, and rapid HPTLC-based method was developed for quantitation of AMT in gastric content of intoxicated patients. Extraction was done from 3 mL gastric lavage sample by liquid-liquid extraction procedure with ethyl acetate-n-heptane (1:1, w / w) in alkaline pH with 10.8. The mobile phase was an isocratic solvent system consisting of methanol-ammonia (25%) (98.5:1.5, v / v). 3,4-Methylenedioxy-Nmethamphetamine (MDMA) was used as internal standard (IS). Analytes were quantified by TLC Scanner operating under 209 nm. The retardation factors of AMT and MDMA were determined as 0.49 and 0.25, respectively. The analytical range was set as 10–250 ng spot−1 for AMT. Calibration was linear within the selected range in gastric lavage (r > 0.9995). Limit of detection and limit of quantification of AMT were found to be 5.1 and 17.3 ng spot−1, respectively. Recoveries of 25 ng spot−1 and 100 ng spot−1 concentrations were found 83.12% and 91.89%; bias% values were 10.91 and 3.19, respectively. The validated method was also applied on samples of five patients who attempted suicide by AMT, and concentrations in gastric lavage samples of 5 patients were found 7.1, 8.3, 9.9, 14.6, and 36.6 ng mL−1. This successfully validated method was applied to suicide cases, and it can be conveniently employed on both antemortem and postmortem cases suspected by amitriptyline.

Human brains found in a fire-affected 4000-years old Bronze Age tumulus layer rich in soil alkalines and boron in Kutahya, Western Anatolia

Undecomposed human bodies and organs always attracted interest in terms of understanding biological tissue stability and immortality. Amongst these, cases of natural mummification found in glaciers, bog sediments and deserts caused even more attention. In 2010, an archeological excavation of a Bronze Age layer in a tumulus near the Western Anatolia city Kütahya revealed fire affected regions with burnt human skeletons and charred wooden objects. Inside of the cracked skulls, undecomposed brains were discernible. To analyze the burial taphonomy of the rare phenomenon of brain preservation, we analyzed brains, bone, teeth and surrounding soils elements using Inductively Coupled Plasma-Mass Spectrometer (ICP-MS). Adipocere formation or saponification of postmortem tissue fat requires high levels of alkalinity and especially potassium. Indeed, ICP-MS analysis of the brain, teeth and bone and also of the surrounding soil revealed high levels of potassium, magnesium, aluminum and boron, which are compatible with the famous role of Kütahya in tile production with its soil containing high level of alkalines and tile-glazing boron. Fatty acid chromatography revealed simultaneous saturation of fats and protection of fragile unsaturated fatty acids consistent with soil-presence of both pro-oxidant and anti-oxidant trace metals. Computerized tomography revealed protection of diencephalic, metencephalic and occipital tissue in one of the best-preserved specimens. Boron was previously found as an intentional preservative of Tutankhamen and Deir el Bahari mummies. Here, in natural soil with its insect-repellant, anti-bacterial and fire-resistance qualities it may be a factor to preserve heat-affected brains as almost bioporcellain specimens.

Madde Kullanımının Kolaylaştırdığı Suçlar: Maddeler ve Etkileri; Deliller ve Analizleri

Deaths by ligature have always been common in the society. The manner of death being suicidal, accidental or homicidal has always been a controversy faced by an autopsy surgeon. Due to the variability of the appearance of the external lesions in different mannerism of mechanical asphyxias the autopsy surgeon is highly dependent upon the history and the circumstances of the death. This study was undertaken in an attempt to identify specific internal lesions in cases of ligature compression of neck. We studied 46 cases of suicidal hanging and 12 cases of ligature strangulation. All the internal lesions were categorized and their correlation was sought in various manner and mode of asphyxia. Strap muscle haemorrhages, laryngeal fractures and tongue bleed were found to be more prevalent in strangulation than hanging. Absence of external injuries points more towards the case being suicidal hanging.

A General Overview of Pesticides in Soil: Requirement of Sensitive and Current Residue Analysis Methods

Pesticides are chemical agents used to destroy or control pests, both in agriculture and in public health. Despite the beneficial effects associated with the usage of them, these chemicals may cause adverse effects to humans and to the nature. In addition, many pesticides are persistent and may therefore bioaccumulate in the environment; also some of them are important carcinogens and mutagens. In the world, alarming levels of pesticides have been detected in air, water, soil, as well as in foods and biological materials. Because of the special character as sink and source of contaminants soil is a critical medium, and as an environmental contaminant that comes into contact with soil intensively, pesticides are one of the important issues of environmental soil forensics. The different classes and wide range of pesticides and environmental mediums containing them have made essential the development of sensitive and current methods for the analysis of pesticide residues for environmental monitoring and forensic investigations. This chapter describes pesticides, historical background of pesticide usage, pesticides classification, environmental impacts and fate of pesticides, misuse and overuse of them, and provides a general brief overview on the soil sampling and pre-treatment, the basic principles of the conventional and also modern extraction approaches (including their advantages and disadvantages), and the chromatographic-based determination techniques used for pesticide residue analysis in soil.